CN105668590B - The absorption process of unreacted ammonia in acrylonitrile reactor device - Google Patents
The absorption process of unreacted ammonia in acrylonitrile reactor device Download PDFInfo
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- CN105668590B CN105668590B CN201410668320.4A CN201410668320A CN105668590B CN 105668590 B CN105668590 B CN 105668590B CN 201410668320 A CN201410668320 A CN 201410668320A CN 105668590 B CN105668590 B CN 105668590B
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Abstract
The present invention relates to the absorption process of unreacted ammonia in acrylonitrile reactor device, mainly solves unreacted ammonia in the prior art and absorbs incomplete problem.By using including：High ammonolysis product air-flow unreacted ammonia in chilling tower contacts the high ammonolysis product air-flow of absorption with poor ammonium absorbing liquid, obtains rich ammonium absorbing liquid and low ammonolysis product air-flow；By rich ammonium absorbing liquid in stripper through stripper stripping gas stripping volatile organic component, supernatant light component is separated off in separator again and is sunken to the heavy constituent of lower floor, then heated in Analytic Tower and Analytic Tower stripping gas strips to obtain thick ammonia flow and poor ammonium absorbing liquid, and poor ammonium absorbing liquid returns to the absorption that chilling tower is used for unreacted ammonia；Thick ammonia flows through ammonia rectifying column rectifying and obtains pure ammonia logistics；Wherein, the technical scheme selected from least one of phosphoric acid, ammonium dihydrogen phosphate or sulfuric acid absorbent is contained in poor ammonium absorbing liquid and preferably solves the problem, available in the commercial plant of acrylonitrile.
Description
Technical field
The present invention relates to the absorption process of unreacted ammonia in acrylonitrile reactor device.
Background technology
10% or so unreacted ammonia is had in Acrylonitrile Production to be needed to be absorbed to isolate from reaction stream
Come.Although there is the content that technology can reduce reactor outlet ammonia, but still there is the presence of a large amount of unreacted ammonia.Production technology at present
Mainly by sulfuric acid scrubbing so as to absorb unreacted ammonia, amine wastewater of sulphuric acid is directly injected into deep-well processing, or through thiamine recovery workshop section
Recovery crystallization sulphur ammonium, or sulphur ammonium are burned and SO are made3, then sulfuric acid is made through absorption and returns system circulation use.Also partial monopoly leads to
In peroxophosphoric acid, ammonium dihydrogen phosphate or the two mixture and recovery unreacted ammonia.
Patent CN1204620A discloses a kind of reaction for being used to from generation alkene nitrile or methacrylonitrile reaction zone obtain
The method of middle recovery unreacted ammonia, above-mentioned reactor effluent is quenched with ammonium phosphate solution after device outflow, wherein, described molten
The ratio between ammonium ion and phosphate anion in liquid are about 0.7-1.3, preferably 1.0-1.2.It is useless remaining in absorbing liquid in order to remove
Organic matter, wet oxidation unit, temperature and 600-3000 of the wet oxidation reaction at about 200 DEG C -650 DEG C are added in method
Pound/square inch pressure under carry out.
Patent CN101027252A discloses a kind of modification method that ammonia is reclaimed and circulated from steam stream, and this method includes
The aqueous solution quenching reaction device effluent of ammonium phosphate is used at least two stages, so as to capture the ammonia components in effluent.It is logical
The ammonia of year capture can be reclaimed by crossing heated phosphoric aqueous ammonium, then circulate the ammonium phosphate solution.Before circulation, by wet
Formula oxidation can remove pollutant contained in ammonium phosphate solution.
But in the prior art, low ammonia production of the high ammonolysis product air-flow from ammonia oxidation reactor after the absorption of poor ammonium absorbing liquid
The ammonia of significant quantity is still remained in product air-flow, so as to influence the raising of product quality.
The content of the invention
The technical problems to be solved by the invention are that unreacted ammonia absorbs incomplete problem in the prior art, there is provided a kind of
The absorption process of unreacted ammonia in new acrylonitrile reactor device.There is this method ammonia to absorb the advantages of complete.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
The absorption process of unreacted ammonia, comprises the following steps in acrylonitrile reactor device：
High ammonolysis product air-flow 6 from ammonia oxidation reactor out contacts absorption height with poor ammonium absorbing liquid 15 in chilling tower 1
Unreacted ammonia in ammonolysis product air-flow, obtain rich ammonium absorbing liquid 8 and low ammonolysis product air-flow 7；
Rich ammonium absorbing liquid 8 is interior through the stripping volatile organic component 10 of stripper stripping gas 9 in stripper 2, then
Supernatant light component 12 is separated off in separator 3 and is sunken to the heavy constituent 13 of lower floor, then through adding in Analytic Tower 4
Heat and the stripping of Analytic Tower stripping gas 14 obtain thick ammonia flow 16 and poor ammonium absorbing liquid 15, and poor ammonium absorbing liquid 15 returns to chilling tower 1 and used
In the absorption of unreacted ammonia；Thick ammonia flow 16 obtains pure ammonia logistics 17 through the rectifying of ammonia rectifying column 5；Wherein, contain in poor ammonium absorbing liquid
Have selected from least one of phosphoric acid, ammonium dihydrogen phosphate or sulfuric acid absorbent.Absorbent in poor ammonium absorbing liquid preferably includes：
(a) at least one of phosphoric acid and ammonium dihydrogen phosphate；Sulfuric acid (b)；S/P mol ratios are 0.01- in more preferably poor ammonium absorbing liquid
0.5, wherein S represent element sulphur, and P represents P elements；Poor ammonium absorbing liquid pH value is preferably 2-6.5 in above-mentioned technical proposal.It is above-mentioned
The mass content of P element is 3%~8% in preferred poor ammonium absorbing liquid 15 in technical scheme.
In above-mentioned technical proposal, separator 3 preferably has the upper outlet of discharge light component 12.
In above-mentioned technical proposal, separator 3 preferably has the lower outlet of discharge heavy constituent 13.
In above-mentioned technical proposal, the temperature of poor ammonium absorbing liquid is preferably 50-85 DEG C.
In above-mentioned technical proposal, stripper stripping gas 9 and/or Analytic Tower stripping gas 14 are preferably inert to stripping thing
Gas.
In above-mentioned technical proposal, the gas inert to stripping thing is preferably at least one in water vapour, air and nitrogen
Kind.
In above-mentioned technical proposal, the heavy constituent 13 is high polymer and/or catalyst fines.
In above-mentioned technical proposal, the poor ammonium absorbing liquid 15 is using water as solvent.
In above-mentioned technical proposal, Analytic Tower temperature is preferably 150-250 DEG C.
In above-mentioned technical proposal, saturated vapor pressure of the pressure tower for solution in the Analytic Tower under relevant temperature is parsed.
In the inventive method before rich ammonium absorbing liquid enters Analytic Tower, without temperature-pressure, polymer is handled, is not required to pass through
The processing of wet oxidation process.And wet oxidation needs to carry out at high temperature under high pressure, energy consumption is higher, causes production cost to raise；Together
When due to operating condition it is harsh, also higher is required to reactor material.So energy consumption can be reduced using this method, production is reduced
Cost.
Place a small amount of sulfuric acid in poor ammonium absorbing liquid in the inventive method, can make the absorption efficiency of ammonia than only with phosphoric acid and/
Or ammonium dihydrogen phosphate is high, also than only using, sulfuric acid is high, and absorptivity reaches 100%, improves the quality of product air-flow.
The present invention is described in detail with reference to the accompanying drawings and detailed description.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
In Fig. 1,1 is chilling tower, and 2 be stripper, and 3 be separator, and 4 be Analytic Tower, and 5 be ammonia rectifying column；6 be that high ammonia produces
Product air-flow, 7 be low ammonolysis product air-flow, and 8 be rich ammonium absorbing liquid, and 9 be stripper stripping gas, and 10 be volatile organic constituents, and 12 are
Light component, 13 be heavy constituent, and 14 be Analytic Tower stripping gas, and 15 be poor ammonium absorbing liquid, and 16 be thick ammonia flow, and 17 be pure ammonia flow.
Flow is shown in Fig. 1：High ammonolysis product air-flow 6 from ammonia oxidation reactor is in chilling tower 1 and poor ammonium absorbing liquid 15
Contact absorbs unreacted ammonia, obtains low ammonolysis product air-flow 7 and rich ammonium absorbing liquid 8, rich ammonium absorbing liquid 8 is in stripper 2 through stripping
Gas 9 removes volatile organic constituents 10, then is separated off supernatant light component 12 in separator 3 and is sunken to lower floor
Heavy constituent 13, it is then heated in Analytic Tower 4 to obtain thick ammonia flow 16 and poor ammonium absorbing liquid with the stripping of Analytic Tower stripping gas 14
15, poor ammonium absorbing liquid 15 returns to chilling tower 1 and is used to circulate the absorption for being used for unreacted ammonia in high ammonolysis product air-flow 6；Thick ammonia flow
16 obtain pure ammonia logistics 17 through the rectifying of ammonia rectifying column 5.
Pure ammonia flow 17 can return to ammonia oxidation reactor (not shown) and be reacted.
Embodiment
Embodiment 1-6 and comparative example 1 and comparative example 2 flow operations as shown in Figure 1, use in poor ammonium absorbing liquid molten
Agent is water.
【Embodiment 1】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.01 in poor ammonium absorbing liquid, and P elements mass content is
6.5%, absorbing liquid pH value is 2, and the temperature of poor ammonium absorbing liquid is 85 DEG C, and ammonia contains in the low ammonolysis product air-flow obtained by absorption
Amount is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after water vapour strips, and removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 195 DEG C, and stripping gas is air.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow exists
Rectifying column obtains high purity anhydrous ammonia after rectifying and returns to acrylonitrile reactor progress ammoxidation reaction.
For ease of comparing, technological condition and result are listed in table 1.
【Embodiment 2】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.05 in poor ammonium absorbing liquid, and P elements mass content is
8.0%, absorbing liquid pH value is 3.5, and the temperature of poor ammonium absorbing liquid is 75 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after air strips, and removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 250 DEG C, and stripping gas is nitrogen.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow exists
Rectifying column obtains high purity anhydrous ammonia after rectifying and returns to acrylonitrile reactor progress ammoxidation reaction.
For ease of comparing, technological condition and result are listed in table 1.
【Embodiment 3】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.1 in poor ammonium absorbing liquid, and P elements mass content is
5.0%, absorbing liquid pH value is 2.5, and the temperature of poor ammonium absorbing liquid is 50 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after nitrogen stripping, removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 150 DEG C, and stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow
High purity anhydrous ammonia is obtained after rectifying in rectifying column and returns to acrylonitrile reactor progress ammoxidation reaction.
For ease of comparing, technological condition and result are listed in table 1.
【Embodiment 4】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.1 in poor ammonium absorbing liquid, and P elements mass content is
6.5%, absorbing liquid pH value is 5.0, and the temperature of poor ammonium absorbing liquid is 80 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after air strips, and removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 190 DEG C, and stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow
High purity anhydrous ammonia is obtained after rectifying in rectifying column and returns to acrylonitrile reactor progress ammoxidation reaction.
For ease of comparing, technological condition and result are listed in table 1.
【Embodiment 5】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.3 in poor ammonium absorbing liquid, and P elements mass content is
6.0%, absorbing liquid pH value is 6.5, and the temperature of poor ammonium absorbing liquid is 65 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after nitrogen stripping, removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 170 DEG C, and stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow
High purity anhydrous ammonia is obtained after rectifying in rectifying column and returns to acrylonitrile reactor progress ammoxidation reaction.
For ease of comparing, technological condition and result are listed in table 1.
【Embodiment 6】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.5 in poor ammonium absorbing liquid, and P elements mass content is
3.3%, absorbing liquid pH value is 5.0, and the temperature of poor ammonium absorbing liquid is 70 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after air strips, and removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 165 DEG C, and stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow
High purity anhydrous ammonia is obtained after rectifying in rectifying column and returns to acrylonitrile reactor progress ammoxidation reaction.
For ease of comparing, technological condition and result are listed in table 1.
【Comparative example 1】
Difference from Example 4 is that the property of poor ammonium absorbing liquid is：S/P mol ratios are 0, pH 5, temperature 80
DEG C, P content 6.5wt%；Other process conditions are same as Example 4.Specially：
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, the content of ammonia is detected as in the low ammonolysis product air-flow obtained by absorption
0.2wt%.Rich ammonium absorbing liquid enters separator in stripper after air strips, remove light component and including catalyst and/
Or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation temperature
For 190 DEG C, stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow is in essence
Evaporate tower and high purity anhydrous ammonia return acrylonitrile reactor progress ammoxidation reaction is obtained after rectifying.
For ease of comparing, technological condition and result are listed in table 1.
【Comparative example 2】
Difference from Example 4 is that the property of poor ammonium absorbing liquid is：Absorbent is sulfuric acid, without P, pH 5, temperature
For 80 DEG C；Other process conditions are same as Example 4.Specially：
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, the content of ammonia is detected as in the low ammonolysis product air-flow obtained by absorption
0.2wt%.Rich ammonium absorbing liquid enters separator in stripper after air strips, remove light component and including catalyst and/
Or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation temperature
For 190 DEG C, stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow is in essence
Evaporate tower and high purity anhydrous ammonia return acrylonitrile reactor progress ammoxidation reaction is obtained after rectifying.
For ease of comparing, technological condition and result are listed in table 1.
Only with the absorbent containing S or only with the absorbent containing P be not so good as using simultaneously the absorbent containing S and P it is good, this from
Comparative example 1 and 2 and embodiment 4 it is year-on-year in can be seen more clearly.
Table 1
Claims (10)
1. the absorption process of unreacted ammonia, comprises the following steps in acrylonitrile reactor device：
High ammonolysis product air-flow (6) from ammonia oxidation reactor out contacts absorption in chilling tower (1) with poor ammonium absorbing liquid (15)
Unreacted ammonia in high ammonolysis product air-flow, obtain rich ammonium absorbing liquid (8) and low ammonolysis product air-flow (7)；
By rich ammonium absorbing liquid (8) in the stripper (2) through stripper stripping gas (9) stripping volatile organic component (10),
Supernatant light component (12) is separated off in separator (3) again and is sunken to the heavy constituent (13) of lower floor, is then being solved
Heated and Analytic Tower stripping gas (14) stripping obtains thick ammonia flow (16) and poor ammonium absorbing liquid (15) in analysis tower (4), and poor ammonium is inhaled
Receive liquid (15) and return to the absorption that chilling tower (1) is used for unreacted ammonia；Thick ammonia flow (16) obtains pure ammonia through ammonia rectifying column (5) rectifying
Logistics (17)；Wherein, absorbent is contained in poor ammonium absorbing liquid, the absorbent includes：(a) in phosphoric acid and ammonium dihydrogen phosphate extremely
Few one kind；Sulfuric acid (b)；S/P mol ratios are 0.01-0.5 in poor ammonium absorbing liquid, and wherein S represents element sulphur, and P represents P elements.
2. according to the method for claim 1, it is characterised in that separator (3) have discharge light component (12) on go out
Mouthful.
3. according to the method for claim 1, it is characterised in that separator (3) has to go out under discharge heavy constituent (13)
Mouthful.
4. according to the method for claim 1, it is characterised in that the temperature of poor ammonium absorbing liquid is 50-85 DEG C.
5. according to the method for claim 1, it is characterised in that stripper stripping gas (9) and/or Analytic Tower stripping gas (14)
For the gas inert to stripping thing.
6. according to the method for claim 5, it is characterised in that the gas inert to stripping thing is water vapour, air and nitrogen
At least one of gas.
7. according to the method described in claim 1, it is characterised in that the heavy constituent (13) is high polymer and/or catalyst fines.
8. according to the method described in claim 1, it is characterised in that the poor ammonium absorbing liquid (15) is using water as solvent.
9. according to the method for claim 1, it is characterised in that Analytic Tower temperature is 150-250 DEG C.
10. according to the method for claim 9, it is characterised in that parsing pressure tower is solution in the Analytic Tower under relevant temperature
Saturated vapor pressure.
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| CN106430245B (en) * | 2015-08-12 | 2018-10-23 | 中国石油化工股份有限公司 | Improved method without thiamine process in acrylonitrile reactor device |
| CN107867747B (en) * | 2016-09-26 | 2020-12-29 | 中国石油化工股份有限公司 | Method for recovering unreacted ammonia in ammonium sulfate-free process in acrylonitrile reaction device |
| CN107866222B (en) * | 2016-09-26 | 2021-05-11 | 中国石油化工股份有限公司 | Ammonium sulfate-free process method in acrylonitrile reaction device |
| CN107126826A (en) * | 2017-04-10 | 2017-09-05 | 天津凯赛特科技有限公司 | Ammonia-contained tail gas treating device and method in prepared by a kind of soda ash |
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| CN102452955A (en) * | 2010-10-21 | 2012-05-16 | 中国石油化工股份有限公司 | Method for recovering and recycling unreacted ammonia in acrylonitrile reaction device |
| CN103420396A (en) * | 2012-05-16 | 2013-12-04 | 中国石油化工股份有限公司 | New method of ammonium salt resolving of ammonium-sulfate-free technology of acrylonitrile |
| CN103729517A (en) * | 2014-01-08 | 2014-04-16 | 西北工业大学 | Dynamics modeling method for space flexible net robot system |
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| CN102452955A (en) * | 2010-10-21 | 2012-05-16 | 中国石油化工股份有限公司 | Method for recovering and recycling unreacted ammonia in acrylonitrile reaction device |
| CN103420396A (en) * | 2012-05-16 | 2013-12-04 | 中国石油化工股份有限公司 | New method of ammonium salt resolving of ammonium-sulfate-free technology of acrylonitrile |
| CN103729517A (en) * | 2014-01-08 | 2014-04-16 | 西北工业大学 | Dynamics modeling method for space flexible net robot system |
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